CN107987966B - Refining process for reducing chloropropanol ester in camellia oil - Google Patents

Refining process for reducing chloropropanol ester in camellia oil Download PDF

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CN107987966B
CN107987966B CN201711103827.5A CN201711103827A CN107987966B CN 107987966 B CN107987966 B CN 107987966B CN 201711103827 A CN201711103827 A CN 201711103827A CN 107987966 B CN107987966 B CN 107987966B
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oil
chloropropanol
reducing
chloropropanol ester
precipitation
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CN107987966A (en
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郑睿行
周华
汪尤刚
祝华明
方春福
周香伦
戴贤君
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Ningbo food inspection and Research Institute
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Quzhou Municipal Center For Disease Control And Prevention
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00Refining fats or fatty oils
    • C11B3/001Refining fats or fatty oils by a combination of two or more of the means hereafter

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  • Microbiology (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract

The invention discloses a refining process for reducing chloropropanol ester in camellia oil, which comprises the following steps: 1) filtering the crude oil, removing mechanical impurities, preheating, adding water for hydration, standing for precipitation, and separating to obtain oil and hydrated oil; adding water into the aqueous oil, adding phosphoric acid, neutralizing with 0.5% liquid sodium silicate, standing for precipitation, and separating oil and soap; 2) putting the crude oil into a decoloring pot to decolor according to a conventional process; 3) deacidifying and deodorizing; heating under low vacuum condition in molecular distillation equipment, and discharging free fatty acid and low molecular odor substance in oil together with steam from distillate; 4) carrying out winterization and dewaxing to obtain a finished product; the invention can not only obviously reduce the content of chloropropanol ester compounds in the tea oil and prevent potential harm of oil products to human bodies, but also ensure that the refined tea oil reaches the national sanitary standard, improve the safety level of the tea oil, provide guarantee for the safety production of the tea oil and provide guarantee for the health of consumers.

Description

Refining process for reducing chloropropanol ester in camellia oil
Technical Field
The invention particularly relates to a refining process for reducing chloropropanol ester in camellia oil.
Background
The chloropropanol ester is an esterification product of chloropropanol compounds and fatty acid, and the ester with higher detection amount of 3-chloropropanol is used in the grease. 3-chloropropanol ester is a potential food safety hazard factor, toxicological research is continuously carried out, and no official report that the 3-chloropropanol ester has direct toxicological effect on human bodies exists at present. However, 3-chloropropanol ester entering the body can be hydrolyzed into free 3-MCPD under the action of intestinal pancreatic lipase, so that the toxic effect is exerted. The 3-MCPD can cause the damage of the liver and the kidney of a mouse, can reduce the sperm activity and the sperm quantity of a rat, inhibit the secretion of male hormone, and reduce the reproductive capacity and even cause sterility. In addition, the metabolite of 3-chloropropanol ester, glycidyl ester, was assigned 2A by the International agency for cancer research, a likely carcinogen. Currently, toxicological studies on 3-chloropropanol esters are mainly based on the hydrolysis of 3-chloropropanol ester to 3-MCPD. The research of the enzymolysis of 3-chloropropanol monoester and 3-chloropropanol diester in intestinal tract model containing pancreatin enzyme has shown that 3-chloropropanol monoester is hydrolyzed to 3-MCPD in 1min in 100% and 3-chloropropanol diester is hydrolyzed to 45%, 65% and 90% separately in 1, 5 and 90 min. In addition, since 3-chloropropanol ester has a structure similar to that of acylglycerol, it is hypothesized that 3-chloropropanol ester may have a metabolic pathway similar to that of acylglycerol in vivo and may be a substrate of lipase, which raises concerns about potential hazards of 3-chloropropanol ester.
At present, no process treatment is available at home and abroad, which can not only remarkably reduce the content of chloropropanol ester compounds in the tea oil, but also can achieve the refining method of the national safety standard of the tea oil.
Disclosure of Invention
The invention aims to provide a refining process for reducing chloropropanol ester in camellia oil, which can remarkably reduce the content of chloropropanol ester compounds in the camellia oil, prevent potential harm of oil products to human bodies, ensure that the refined camellia oil reaches the national hygienic standard, improve the safety level of the camellia oil, provide guarantee for the safe production of the camellia oil and provide guarantee for the health of consumers.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a refining process for reducing chloropropanol ester in camellia oil comprises the following steps:
1) filtering the crude oil, removing mechanical impurities, preheating, adding water for hydration, standing for precipitation, and separating to obtain oil and hydrated oil; adding water into the aqueous oil, adding phosphoric acid, neutralizing with 0.5% liquid sodium silicate, standing for precipitation, and separating oil and soap;
2) putting the crude oil into a decoloring pot to decolor according to a conventional process;
3) deacidifying and deodorizing; heating under low vacuum condition in molecular distillation equipment, and discharging free fatty acid and low molecular odor substance in oil together with steam from distillate;
4) dewaxing in winterization to obtain the finished product.
Further, in the step 1), the preheating temperature is 30-50 ℃, and the water adding amount during hydration is 10% of the total amount of the crude oil.
Further, in the step 1), the amount of the added phosphoric acid is 0.05 percent of the total amount of the hydrated oil, the mass concentration of the phosphoric acid is 85 percent, and the amount of the added liquid sodium silicate is 0.5 percent of the total amount.
Further, in the step 3), the adopted molecular distillation equipment is a centrifugal molecular distillation device, the vacuum condition is 0.5 Pa-1 Pa, and the heating temperature is 165 ℃.
The technical effects of the invention are mainly reflected in the following aspects: the method improves the traditional tea oil refining process, firstly, the salting-out agent is not used in hydration, and the source of chloride ions is controlled and reduced from the source; secondly, decoloring and deacidifying to neutralize non-hydrophilic colloid substance to improve degumming effect; thirdly, the deacidification by molecular distillation replaces the deacidification by alkali refining, so that the use of NaOH is controlled, and the pollution of chloride ions is reduced to a certain extent; fourthly, deacidifying and deodorizing are synchronously completed, the separation degree and the yield are high, the product quality is high, the components of the product are not changed too much before and after distillation, and the fractionation process of molecular distillation is a physical process, so that the separated substances can be well protected from being polluted and damaged.
Detailed Description
In the present embodiment, it should be noted that the relational terms such as first and second, and the like are only used for distinguishing one entity or operation from another 4 entities or operations, and do not necessarily require or imply any actual relationship or order between the entities or operations. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
In addition, in the present embodiment, if the connection or fixing manner between the components is not specifically described, the connection or fixing manner may be a bolt fixing manner, a pin fixing manner, or a pin shaft connecting manner, which is commonly used in the prior art, and therefore, detailed description thereof is omitted in this embodiment.
Examples
A refining process for reducing chloropropanol ester in camellia oil comprises the following steps:
1) filtering crude oil containing a small amount of colloid, filtering to remove mechanical impurities, preheating, adding water for hydration, standing for precipitation, and separating to obtain oil and hydrated oil; adding water into the aqueous oil, adding phosphoric acid instead of salt, reducing C l sources, neutralizing non-hydrophilic colloid substance to improve degumming effect, neutralizing with 0.5% liquid sodium silicate, standing for precipitation, and separating oil and soap;
2) putting the crude oil into a decoloring pot for decoloring, and performing in the decoloring pot according to a conventional process;
3) deacidifying and deodorizing; heating in molecular distillation equipment under low vacuum condition, escaping from condensation surface by virtue of difference of free stroke of each component in crude oil, and discharging free fatty acid and low molecular odor substance in oil together with steam by fraction;
4) dewaxing in winterization to obtain the finished product.
In the step 1), the preheating temperature is 30-50 ℃, and the water adding amount during hydration is 10% of the total amount of the crude oil.
In the step 1), the added phosphoric acid accounts for 0.05 percent of the total amount of the hydrated oil, the mass concentration of the phosphoric acid is 85 percent, and the added liquid sodium silicate accounts for 0.5 percent of the total amount.
In the step 3), the adopted molecular distillation equipment is a centrifugal molecular distillation device, the vacuum condition is 0.5 Pa-1 Pa, and the heating temperature is 165 ℃.
Experimental example:
the oil prepared by the method not only meets the edible oil sanitary standard GB2716-2005, but also has the following table advantages (the number of samples n is 9)
Figure BDA0001463779410000041
Figure BDA0001463779410000051
Therefore, the chloropropanol produced by the process of the invention is obviously reduced.
Description of the principle:
salt salting-out is avoided during hydration, and the source of chloride ions is controlled and reduced from the source; the molecular distillation is used for replacing alkali refining, so that the use of NaOH is controlled, and the pollution of chloride ions is reduced to a certain extent; the distillation temperature is low. Ordinary distillation is carried out at the boiling point temperature, molecular distillation is carried out at any temperature lower than the boiling point of the distillation substance, and the separation can be achieved as long as the temperature difference exists between the substances to be separated. A key link of chloropropanol ester steep increase caused by high-temperature deodorization is controlled; the distillation vacuum degree is high. The whole material system is under vacuum, and the lowest distillation pressure of the material system is required to be lower than 0.5 Pa-1 Pa, so that the material is not easy to oxidize and damage, and the stability of fatty acid in the tea oil is ensured; the heating time is short. The distance between the heating surface and the condensing surface of the molecular distillation device is less than the mean free path of the light molecules, and the light molecules escaping from the liquid surface reach the condensing surface almost without collision, so the heating time is very short, and the retention time at the distillation temperature is generally between a few seconds and a few tens of seconds. The molecular distillation temperature is low, the heating time is short, and the tea oil is prevented from being oxidized by the processing environment; high efficiency and safety. High separation degree and yield, high product quality, and no great change of components before and after distillation. The fractionation process of molecular distillation is a physical process and thus provides good protection against contamination and attack of the separated material. The separated product is non-toxic, harmless, pollution-free and residue-free, and a pure and safe product can be obtained.
The technical effects of the invention are mainly reflected in the following aspects: the method improves the traditional tea oil refining process, firstly, the salting-out agent is not used in hydration, and the source of chloride ions is controlled and reduced from the source; secondly, decoloring and deacidifying to neutralize non-hydrophilic colloid substance to improve degumming effect; thirdly, the deacidification by molecular distillation replaces the deacidification by alkali refining, so that the use of NaOH is controlled, and the pollution of chloride ions is reduced to a certain extent; fourthly, deacidifying and deodorizing are synchronously completed, the separation degree and the yield are high, the product quality is high, the components of the product are not changed too much before and after distillation, and the fractionation process of molecular distillation is a physical process, so that the separated substances can be well protected from being polluted and damaged.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that are not thought of through the inventive work should be included in the scope of the present invention.

Claims (2)

1. A refining process for reducing chloropropanol ester in camellia oil is characterized by comprising the following steps:
1) filtering the crude oil, removing mechanical impurities, preheating, adding water for hydration, standing for precipitation, and separating to obtain oil and hydrated oil; adding water into the aqueous oil, adding phosphoric acid, neutralizing with 0.5% liquid sodium silicate, standing for precipitation, and separating oil and soap;
2) putting the crude oil obtained by the oil soap separation in the step 1) into a decoloring pot, and decoloring according to a conventional process;
3) deacidifying and deodorizing; heating under low vacuum condition in molecular distillation equipment, and discharging free fatty acid and low molecular odor substance in oil together with steam from distillate;
4) carrying out winterization and dewaxing to obtain a finished product;
in the step 1), the preheating temperature is 30-50 ℃, and the water adding amount during hydration is 10% of the total amount of the crude oil;
in the step 3), the adopted molecular distillation equipment is a centrifugal molecular distillation device, the vacuum condition is 0.5 Pa-1 Pa, and the heating temperature is 165 ℃.
2. The refining process for reducing chloropropanol ester in camellia oil as claimed in claim 1, wherein: in the step 1), the added phosphoric acid accounts for 0.05 percent of the total amount of the hydrated oil, the mass concentration of the phosphoric acid is 85 percent, and the added liquid sodium silicate accounts for 0.5 percent of the total amount.
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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103382413A (en) * 2013-07-16 2013-11-06 傅武胜 Refining process for reducing content of MCPD in tea seed oil

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103382413A (en) * 2013-07-16 2013-11-06 傅武胜 Refining process for reducing content of MCPD in tea seed oil

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